The Isothermal and Nonisothermal Crystallization Kinetics and Morphology of Solvent-Precipitated Nylon 66
Abstract
:1. Introduction
2. Experimental Section
2.1. Material and Sample Preparation
2.2. Differential Scanning Calorimetry (DSC)
2.3. Isothermal and Nonisothermal Crystallization Process
2.4. Polarized Optical Microscopy (POM)
2.5. X-ray Diffraction (XRD)
3. Results and Discussion
3.1. Isothermal Crystallization Kinetics from Avrami Equation
3.2. Isothermal Crystallization Activation Energy (ΔE)
3.3. Nonisothermal Crystallization Behaviors
3.3.1. Modified Avrami Equation by Jeziorny
3.3.2. Modified Avrami Equation by Ozawa
3.3.3. The Mo Method
3.4. Crystallization Activation Energy ΔE
3.5. Crystallite Morphology
3.6. Characterization of Solvent-Precipitated Nylon 66
4. Conclusions
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Conflicts of Interest
References
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Sample | Tc (°C) | n | K(min−1) | tmax (min) | t1/2 (min) | τ1/2 (min−1) | X(tmax) (%) |
---|---|---|---|---|---|---|---|
PA66-BP | 219 | 2.406 | 0.782 | 1.267 | 1.360 | 0.732 | 41.83 |
221 | 2.490 | 0.402 | 1.700 | 1.706 | 0.586 | 49.60 | |
223 | 2.730 | 0.160 | 2.150 | 2.380 | 0.447 | 45.52 | |
225 | 2.813 | 0.052 | 3.067 | 3.116 | 0.321 | 48.13 | |
227 | 2.838 | 0.016 | 4.333 | 4.356 | 0.230 | 49.42 | |
PA66-NU | 219 | 2.341 | 10.35 | 0.467 | 0.529 | 1.890 | 34.50 |
221 | 2.299 | 7.963 | 0.517 | 0.576 | 1.736 | 36.81 | |
223 | 2.403 | 6.126 | 0.567 | 0.632 | 1.582 | 37.00 | |
225 | 2.374 | 4.206 | 0.633 | 0.712 | 1.405 | 36.55 | |
227 | 2.338 | 3.061 | 0.717 | 0.808 | 1.238 | 36.52 | |
PA66-FA | 219 | 2.551 | 140.8 | 0.100 | 0.124 | 8.065 | 33.57 |
221 | 2.477 | 78.67 | 0.167 | 0.181 | 5.525 | 42.22 | |
223 | 2.255 | 22.25 | 0.400 | 0.431 | 2.320 | 38.93 | |
227 | 2.228 | 9.343 | 0.433 | 0.508 | 1.969 | 32.00 | |
229 | 2.236 | 3.017 | 0.633 | 0.761 | 1.314 | 31.52 | |
PA66-HS | 221 | 2.888 | 355.3 | 0.200 | 0.215 | 4.651 | 29.98 |
223 | 2.952 | 94.45 | 0.300 | 0.321 | 3.115 | 29.44 | |
227 | 2.654 | 25.35 | 0.467 | 0.490 | 2.041 | 42.33 | |
229 | 2.751 | 3.030 | 0.800 | 0.882 | 1.134 | 37.66 | |
231 | 2.842 | 0.340 | 1.450 | 1.675 | 0.597 | 34.28 | |
PA66-MC | 219 | 2.359 | 12.91 | 0.417 | 0.452 | 2.212 | 39.06 |
221 | 2.416 | 4.996 | 0.467 | 0.507 | 1.972 | 39.47 | |
223 | 2.277 | 1.968 | 0.500 | 0.553 | 1.808 | 37.96 | |
227 | 2.122 | 1.045 | 0.567 | 0.628 | 1.592 | 38.89 | |
229 | 2.141 | 1.968 | 0.767 | 0.882 | 1.134 | 36.63 |
Sample | Φ (°C/min) | T* (°C) | tmax (min) | X(t) (%) |
---|---|---|---|---|
PA66-BP | 2.5 | 221.95 | 5.22 | 61.71 |
5 | 215.75 | 4.10 | 69.06 | |
10 | 210.33 | 2.12 | 66.76 | |
20 | 203.32 | 1.26 | 61.40 | |
40 | 193.30 | 0.72 | 59.22 | |
PA66-NU | 2.5 | 237.12 | 5.17 | 57.12 |
5 | 232.16 | 1.30 | 33.03 | |
10 | 225.83 | 0.89 | 43.95 | |
20 | 218.32 | 0.55 | 46.63 | |
40 | 209.30 | 0.35 | 43.21 | |
PA66-FA | 2.5 | 228.87 | 2.47 | 29.34 |
5 | 222.50 | 1.37 | 35.81 | |
10 | 217.16 | 0.81 | 41.11 | |
20 | 211.98 | 0.50 | 37.90 | |
40 | 204.63 | 0.30 | 37.87 | |
PA66-HS | 2.5 | 236.95 | 3.05 | 50.00 |
5 | 236.01 | 1.10 | 44.20 | |
10 | 232.53 | 0.70 | 39.21 | |
20 | 227.98 | 0.38 | 39.81 | |
40 | 222.63 | 0.23 | 42.20 | |
PA66-MC | 2.5 | 225.95 | 5.45 | 48.19 |
5 | 220.91 | 2.59 | 50.22 | |
10 | 218.49 | 1.37 | 47.64 | |
20 | 213.32 | 0.72 | 50.00 | |
40 | 205.97 | 0.35 | 50.33 |
Primary Crystallization Stage | Secondary Crystallization Stage | ||||||
---|---|---|---|---|---|---|---|
Sample | n1 | Zt1 | Zc1 | n2 | Zt2 | Zc2 | |
PA66-BP | 2.5 | 3.012 | 0.006 | 0.130 | 5.520 | 0.0001 | 0.025 |
5 | 3.449 | 0.008 | 0.379 | 6.426 | 0.0001 | 0.167 | |
10 | 4.036 | 0.049 | 0.740 | 6.221 | 0.009 | 0.627 | |
20 | 4.306 | 0.335 | 0.947 | 4.759 | 0.344 | 0.948 | |
40 | 4.130 | 3.387 | 1.031 | 3.499 | 3.474 | 1.032 | |
PA66-NU | 2.5 | 3.202 | 0.005 | 0.121 | 1.663 | 0.058 | 0.321 |
5 | 3.518 | 0.176 | 0.706 | 1.587 | 0.464 | 0.858 | |
10 | 3.723 | 0.906 | 0.990 | 1.329 | 1.215 | 1.020 | |
20 | 3.848 | 6.124 | 1.095 | 1.307 | 2.352 | 1.044 | |
40 | 3.941 | 34.74 | 1.093 | 1.453 | 4.541 | 1.039 | |
PA66-FA | 2.5 | 3.690 | 0.017 | 0.169 | 1.660 | 0.137 | 0.451 |
5 | 3.232 | 0.151 | 0.686 | 1.563 | 0.401 | 0.833 | |
10 | 4.196 | 1.185 | 1.017 | 1.258 | 1.126 | 1.012 | |
20 | 4.306 | 8.644 | 1.114 | 1.250 | 1.854 | 1.031 | |
40 | 4.226 | 69.167 | 1.112 | 1.225 | 3.484 | 1.032 | |
PA66-HS | 2.5 | 7.531 | 0.015 | 0.030 | 3.007 | 0.039 | 0.274 |
5 | 5.044 | 0.355 | 0.813 | 1.005 | 1.012 | 1.003 | |
10 | 6.227 | 4.465 | 1.161 | 0.943 | 1.803 | 1.061 | |
20 | 4.922 | 54.06 | 1.221 | 0.983 | 3.111 | 1.058 | |
40 | 4.187 | 235.2 | 1.146 | 0.964 | 4.672 | 1.039 | |
PA66-MC | 2.5 | 4.358 | 0.001 | 0.044 | 1.760 | 0.056 | 0.316 |
5 | 4.149 | 0.014 | 0.424 | 2.402 | 0.104 | 0.635 | |
10 | 3.881 | 0.191 | 0.848 | 1.338 | 0.765 | 0.974 | |
20 | 3.749 | 2.416 | 1.050 | 1.345 | 1.969 | 1.035 | |
40 | 3.633 | 22.91 | 1.080 | 2.211 | 8.482 | 1.055 |
Sample | Xt (%) | a | F(T) |
---|---|---|---|
PA66-BP | 20 | 1.284 | 17.28 |
40 | 1.251 | 22.39 | |
50 | 1.246 | 24.34 | |
60 | 1.246 | 26.19 | |
80 | 1.250 | 30.10 | |
PA66-NU | 20 | 1.507 | 5.536 |
40 | 1.489 | 7.716 | |
50 | 1.474 | 8.802 | |
60 | 1.455 | 10.04 | |
80 | 1.383 | 14.16 | |
PA66-FA | 20 | 1.292 | 6.390 |
40 | 1.252 | 9.266 | |
50 | 1.245 | 10.45 | |
60 | 1.264 | 12.39 | |
80 | 1.351 | 24.09 | |
PA66-HS | 20 | 1.282 | 4.820 |
40 | 1.320 | 6.023 | |
50 | 1.336 | 6.694 | |
60 | 1.354 | 7.556 | |
80 | 1.389 | 11.08 | |
PA66-MC | 20 | 1.025 | 10.53 |
40 | 1.040 | 13.10 | |
50 | 1.046 | 14.23 | |
60 | 1.050 | 15.36 | |
80 | 1.055 | 18.21 |
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Tseng, C.-H.; Tsai, P.-S. The Isothermal and Nonisothermal Crystallization Kinetics and Morphology of Solvent-Precipitated Nylon 66. Polymers 2022, 14, 442. https://doi.org/10.3390/polym14030442
Tseng C-H, Tsai P-S. The Isothermal and Nonisothermal Crystallization Kinetics and Morphology of Solvent-Precipitated Nylon 66. Polymers. 2022; 14(3):442. https://doi.org/10.3390/polym14030442
Chicago/Turabian StyleTseng, Chiah-Hsiung, and Ping-Szu Tsai. 2022. "The Isothermal and Nonisothermal Crystallization Kinetics and Morphology of Solvent-Precipitated Nylon 66" Polymers 14, no. 3: 442. https://doi.org/10.3390/polym14030442